Process of treating vegetable fibers in the presence of organic derivatives of cellulose



Patented Aug. 27, 1929.

UNI-TED STATES'PATENT OFFICE.

CAMILLE DREYFUS AND ROBERT G. DORT, OF -NEW YORK, N. Y., AND HERBERT PLATT, F CUMBERLAND, MARYLAND, ASSIGNORS TO CELANESE CORPORATION OF AMERICA, A CORPORATION OF DELAWARE.

PROCESS OF TREATING VEGETABLE FIBERS IN THE PRESENCE OF ORGANIC DERIVA- TIVES OF CEI-LULOSE.

No Drawing. Application filed July 8,

This invention relates to the carbonization of vegetable fibers in fabrics and other articles containing fibers or threads of cellulose acetate, cellulose proportionate or other organic esters or ethers of cellulose. It also relates to the treatment of fibers and articles of the above mentioned organic derivatives of cellulose so that they will be able to undergo the carbonization treatment, herein after described, without impairment of their valuable dyeing, dye resist and weaving qualities, nor be affected in their appearance as a result of this treatment. Another important application of this invention is the utilization, in the embroider industry, of this property in materials ma e from organic derivatives of cellulose to resist carbonization treatment.

As a result of our investigations we have discovered that fibers of organic cellulose. esters and cellulose ethers are unaffected by the usual carbonization of vegetable fibers. This is contrary to what has generally been believed and different from what one would normally expect. Rayon or silk,- of the regenerated cellulose type, is completely removed by such carbonizing treatment and this treatment is, therefore, of great'utilityin removing this brand of silk and vegetable fibers from wool waste and woolen rags or other animal fibers.

Heretofore it has been thought that only real or natural silk could be usedin mixed fabrics to obtain a striped or twocolor efiect because of the ease with which rayon of the regenerated cellulose type was-removed by carbonization treatment. Our investigations have shown that fibers or threads made from cellulose acetate or other organic esters or ethers can .be successfully used as a substitute for real silk to obtain such effects. In fact the wearing, dying and dye'resist properties of such fibers or threads are less affected by the carbonization treatment than are the similar properties of real or natural silk. The lustre of-fibers of cellulose acetate or 7 other organic derivatives of cellulose is not, or, at worst, but very slightly affected by the carbonization treatment, nor are their.

dyeing and dye resisting properties impaired. Cross dyeing and bi-color' dyeing will still give the same brilliant ,and clean 1926. Serial No. 121,266.

effects obtained with such mixed fabrics or fibers prior'to carbonization. Where there has been a slight delustering of the cellulose acetate, etc., fibers, and it is considered desirable to reluster the same, this can be accomplished by a slight soaping of the fabric or fibers.

When it is desired to prevent the delustering of the cellulose acetate, or similar fibers, rather than to reluster the same as above set out, this can be accomplished b taking the following precautions. The ad ition of varying amounts of Glaubers salt to the carbon'izing bath will prevent the slight delustering of the cellulose acetate fibers or threads, which delustering is probably due to the deposition of aluminum oxide, when aluminum chloride is used in the carbonizing treatment, on the fiber of cellulose acetate or "other organic derivatives of cellulose. The addition of Glaube'rs salt permits the boiling of the solution without the resultant deposition of alumina on the fabric.

Where it is desired to dye the wool of a mixed fabric containing wool and fibers of organic esters of cellulose after the carbonization and the subsequent soaping, this can be accomplished by dyeing the goods with.

dye-stuffs for wool, which normally do not stain cellulose acetate, etc. from an acetic acid or formic acid bath. This is possible by virtue of the fact that the dye resist.

properties of the cellulose acetate, etc. are unaltered by the carbonization treatment.

Delustering of the fiber or fibers of cellulose acetate or other organic esters or ethers of cellulose, due to high temperatures used in any of the treatments such as bleaching, dyeing, printing, steaming, etc., can be prevented by the addition of Glaubers salt to the bath or baths. The quantity of salt added will determine the length of time which the cellulose acetate, etc. can be'heated at high temperatures or boiled without delustering taklng place. Thus the addition of 5,0 grams'of anhydrous Glaubers salt to a litre of bath will permit the cellulose acetate containing fabric to be treated in the bath at a temperature from 90 C. to boiling for 5 to 7 minutes without becoming delustered. The addition of 150 to 200 grams of anhydrous Glaubers salt to a litre of bath will ermit such a fabric to be similarly treated For a period of 25 to 35 minutes without any delustering of the cellulose acetate portion resulting. The addition of 250. to 300 grams of anhydrous Glaubers salt per litre of bath will enable the boiling treatment to continue for an hour and hour and an a half without any delustering of the cellulose acetate portion of the fabric. Instead of using Glauberssalt as a delustering preventative any of the salts enumerated in U. S. patent application 15,416, filed July 22nd, 1925, can be employed. Among the salts mentioned in said application are the bromide, chromate, oxalate, nitrate, phosphate and sulfate of ammonium; alum; the bichromate, sulfite, dibasic phosphate, nitrite, bisulfite, acetate, thiosulfate, ferrocyanide, chlorate, nitrate, chloride, sulfate, hydrosulfite, sulfite, tartrate and bromide of sodium, calcium chloride; cadmium chloride, copper sulfate, chrome alum; ferrous ammonium sulfate; strontium chloride; the chromate, ferrocyanide, sulfate, chloride, sulfite, nitrate, oxalate, dibasic phosphate and nitrite of potassium; the sulfate and chloride of zinc; tartar emetic; ferrous sulfate; iron alum; barium chloride; the chloride and sulfate of magnesium; aluminum chloride; magnesium nitrate; and orthoaminophenol para sulphonic acid. The amounts of such salts to be used will, of course, differ from the amounts of Glaubers salt above indicated. The equivalent amounts of the different salts which can be used in place of Glaubers salt are set out in the U. S. patent application 15, 11 6, above referred to.

As stated above, the treatment to carbonize vegetable fibers in mixed woolen fabrics of cellulose acetate, cellulose butyrate, etc. does not affect the latter. By the term vegetable fibers, as used in the specification and claims, we include cotton, all artificial silks of the regenerated cellulose type, linen, jute, hemp, etc. or any other fiber of vegetable origin. By the term animal fiber, we include wool, silk or any other fiber having animal origin. By carbonizing processes we refer to the treatments with aluminum chloride, hydrochloric acid and sulphuric acid to remove vegetable fibers.

For illustrative purposes only we give the following examples of how the carbonization may be carried out:

Ewample 1.A woolen fabric containing.

vegetable fibers as well as fibers of cellulose acetate or fibers of other organic esters or others is treated in a solution of aluminum chloride of 6 to 13 B. at 90 F. The excess of aluminum chloride solution is then removed by pressing or squeezing the fabric on a jig after which the fabric is hydroextracted. After hydro-extraction the fab- IlC is passed thru, a carbonizing dryer at 235 F., the fabric coming out bone dry. In

this process, as outlined, there may result a slight delustering of the fabric of the or ganic derivatives of cellulose due to the deposition of aluminum oxide on the surface. This can be removed by a soaping treatment. The above process results in all vegetable fibers being removed, leaving only the wool and cellulose derivatives fibers.

This unique property, that is the resistance to carbonization, of the organic derivatives of cellulose is of great importance in the production 'of embroidery from cellulose acetate and similar fibers. The cellulose acetate or similar fibers are used to em-- broider on a cotton or jute canvas. As heretofore practiced, the cotton or jute canvas is then removed either by hand or by mechanical means, a tedious and costly operation. By virtue of our discovery of the resistance of cellulose acetate and similar fibers to carbonization, it is now possible to remove the canvas by chemical treatment. This results not only in a superior product but also effects a considerable savin in time and labor. The following exampl e of the application of the process as applied to the embroidery industry, is merely illustrative and the invention is not to be considered as limited thereto.

E sample 2.The embroidery made from fibersof cellulose acetate or other organic esters or others of cellulose on a background of cotton canvas is passed thru a bath of 1 to 2% hydrochloric acid at 120 F. The excess acid solution is then squeezed'out and the fabric slightly hydroextracted. The thus treated material is then passed thru a carbonizing dryer maintained at a temperature of 240 F. After the carbonization the fabric is rinsed and given a scouring treatment with soap. This carbonizing treatment removes the cotton background but leaves the cellulose derivative fibers unaffected.

Other uses or applications of this class of fibers, as a result of the discovery of this valuable property, will suggest themselves to those skilled in the art. Thus, for example, such fibers can be used in the manufacture of womens dress goods from woolen to remove the vegetable matter. Also it enables striped and multi-color effects to be obtained without the use of real silk.

Having described our invention what we claim and desire to secureby Letters Patcut is:

process for the treatment of mixed fabrics containing organic derivatives of cellulose and vegetable fibers which comprises subjecting said fabric to the action of a carbonizing solution, whereby the vege table fibers are rendered removable 2. A process for the treatment of mixed fabrics waste or shoddy which must be carbonized containing animal fibers, organic derivatives of cellulose and vegetable fibers which comprises subjecting said fabric to the action of a carbonizing solution, whereby the vegetable fibers are rendered removable.

3. A process'for the treatment of mixed fabrics of wool, organic derivatives of cellulose and vegetable fibers which comprises subjecting said fabric to the action of a carbonizing solution, whereby the vegetable fibers are rendered removable.

4. A process of treating mixed fabrics containing wool, organic esters of cellulose and vegetable fibers which comprises subjecting said fabric to the action of a carbonizing solution, whereby the vegetable fibers are rendered removable.

5. A process for the treatment of mixed fabrics containing wool, cellulose acetate and vegetable fibers which comprises subjecting said fabric to the action of a carbonizing solution, whereby the vegetable fibers are rendered removable.

6. A process of treating mixed fabrics containing wool, organic esters of cellulose and vegetable fibers which comprises subjecting the fabric to the action of an aluminum chloride solution at 90 F., removing the excess of the solution, then drying the treated material in a carbonizing dryer at 235 F., whereby all the vegetable fibers are rendered removable.

7. A process of treating mixed fabrics con taining wool, cellulose acetate and vegetable fibers which comprises subjecting said fabric to the action of an aluminum chloride solution at 90 F., removing the excess of the solution, then drying the treated material in a carbonizing dryer at 235 F whereby the vegetable fibers are rendered removable.

8'. A process oftreating mixed fabrics containing wool,,ecllulose acetate and vegetable fibers which comprisessubjecting said fabric to the action of a 6 to 13 B. solution of aluminum chloride at 90 F., removing the excess of the aluminum chloride solution, then drying the treated material in a carbonizing dryer at 235 F., whereby the vegetable fibers are rendered removable.

9. A process for the treatment of mixed fabrics of organic esters of cellulose, wool and vegetable fibers, which cbmprises subjecting said fabric to the action of a 6 to 13 B. solution of aluminum chloride at 90 F., removing the excess of the solution, drying the treated material in a carbonizing dryer at 235 F., drying and removing the vegetable fibers and finally subjecting the material to a soaping treatment to restore the lustre of the fibers of the organic derivatives of cellulose.

10. A process of'treating mixed fabrics containing cellulose acetate, wool and vegetable fibers which comprises subjecting said fabric to the action of a 6 to 13 B. solution of aluminum chloride at 90 F removing the excess of the aluminum chloride solution, drying the treated material in a carbonizing dryer at 235 F., removing all of the vegetable fibers and finally subjecting the material to a soaping treatment to restore the lustre of the cellulose acetate fibers.

11. In the process of treating a mixed fabric containing organic .esters of cellulose and vegetable fibers, the step of treating said' fabric with a carbonizing solution containlng a luster protective agent for said orgamc ester of cellulose.

12. In the process of treating a mixed fab- I ric containing cellulose acetate and vegetable fibers, the step of treating said fabric with a carbonizing solution containing a luster protective agent for said cellulose acetate.

13. In the process of treating a mixed fabric containing organic esters of cellulose and vegetable fibers, the step of treating said fabric with a carbonizing solution containing Glaubers salt.

14. In the process of treating a mixed fabric containing cellulose acetate and vegetable fibers, the step of treating said fabric with a carbonizing solution containing Glaubers salt.

' In testimony whereof, we have hereunto subscribed ournames.

CAMILLE DREYFUS. ROBERT G. DORT. HERBERT PLATT. 

